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建立了基于脂肪酸的漂浮液滴固化分散液液微萃取(FA-DLLME-SFO)方法,与高效液相色谱联用检测了酒类样品中的4-乙基苯酚和4-乙基愈创木酚。该方法萃取时间仅需4 min,仅需脂肪酸、氨水和硫酸3种对环境友好的试剂。对影响方法萃取效率的因素(包括样品的体积、萃取剂的种类和用量、氨水和硫酸的体积以及盐的加入量)进行了详细的考察。在最佳萃取条件下(10 mL样品,100μL辛酸萃取剂,110μL 25%~28%(质量分数)的氨水,0.8 mL 98%(质量分数)的浓硫酸,3.0 g NaCl),4-乙基苯酚和4-乙基愈创木酚在0.02~1.0 mg/L范围内呈良好的线性关系,相关系数分别为0.999 7和0.999 9,相对标准偏差(n=3)分别为6.2%和3.5%,检出限分别为6.33和5.81μg/L,富集倍数分别为79和86。在啤酒和白葡萄酒样品中,加标回收率为81.4%~108.7%,相对标准偏差(n=3)小于8.9%。该方法简单、对环境友好,可用于酒类样品中4-乙基苯酚和4-乙基愈创木酚的检测。
A FA-DLLME-SFO method was developed for the determination of 4-ethylphenol and 4-ethyl guaiac in alcohol samples by HPLC. phenol. The extraction time of this method is only 4 min, only three kinds of environmentally friendly reagents of fatty acids, ammonia and sulfuric acid are needed. Factors affecting extraction efficiency of the method, including the volume of the sample, the type and amount of extractant, the volume of ammonia and sulfuric acid and the amount of salt added, were investigated in detail. Under the optimal extraction conditions (10 mL sample, 100 μL octanoic acid extractant, 110 μL ammonia water of 25-28% by mass, 0.8 mL concentrated sulfuric acid of 98 mass%, 3.0 g NaCl), 4-ethyl There was a good linear relationship between phenol and 4-ethyl guaiacol in the range of 0.02-1.0 mg / L with the correlation coefficients of 0.999 7 and 0.999 9, respectively. The relative standard deviations (n = 3) were 6.2% and 3.5% The detection limits were 6.33 and 5.81 μg / L, respectively. The enrichment factors were 79 and 86, respectively. In beer and white wine samples, spiked recoveries ranged from 81.4% to 108.7% with relative standard deviations (n = 3) of less than 8.9%. The method is simple and environment-friendly, and can be used for the detection of 4-ethylphenol and 4-ethyl guaiacol in wine samples.